CN106966388A - A kind of micro crystal graphite high-temperature fluorination method of purification - Google Patents

A kind of micro crystal graphite high-temperature fluorination method of purification Download PDF

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Publication number
CN106966388A
CN106966388A CN201710293844.3A CN201710293844A CN106966388A CN 106966388 A CN106966388 A CN 106966388A CN 201710293844 A CN201710293844 A CN 201710293844A CN 106966388 A CN106966388 A CN 106966388A
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China
Prior art keywords
micro crystal
graphite
crystal graphite
purification
temperature
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CN201710293844.3A
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Chinese (zh)
Inventor
林锋
余常伟
张杨健
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Fujian Kai Yu Microcrystalline Graphite Co Ltd
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Fujian Kai Yu Microcrystalline Graphite Co Ltd
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Priority to CN201710293844.3A priority Critical patent/CN106966388A/en
Publication of CN106966388A publication Critical patent/CN106966388A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

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Abstract

The invention discloses a kind of micro crystal graphite high-temperature fluorination method of purification, the natural micro crystal graphite that fixed carbon is 99.9% is taken, fluorization agent is added, delivers to and pyroreaction is carried out in serialization high temperature furnace, the natural micro crystal graphite that purity is more than 99.900% is obtained;The present invention uses fluorization agent and serialization high temperature furnace, the purification graphite of fixed carbon 99.9% to the graphite of fixed carbon 99.990 99.999%.

Description

A kind of micro crystal graphite high-temperature fluorination method of purification
Technical field
The present invention relates to the purification technique field of micro crystal graphite, more particularly to a kind of micro crystal graphite high-temperature fluorination purification side Method.
Background technology
Micro crystal graphite has very important ground in some special industries or high-tech area as a kind of raw material of industry Position, such as atomic energy industry, auto industry, space technology, biotechnology industry.Its is carbon containing for the micro crystal graphite that these industries are used Amount must be more than 99.9% high-purity micro crystal graphite, and the phosphorus content of the natural micro crystal graphite after general ore dressing is up to 80% or so, by commonly reaching 99.5% after alkali fusion/pickling, the requirement using high-purity industry can not be much met, is this Must be to the further purification of micro crystal graphite.
A kind of Patent No. 200910112366.7, entitled purification of microcrystalline graphite product makes new technology with purifying, Comprise the following steps:Reach that mog is to add quick lime in the graphite raw ore that -200 mesh percent of pass are more than 90% in fine grinding Stirred with water, make the pH of the graphite ore pulp containing quick lime>9, waterglass stirring, kerosene stirring are added, pine camphor is eventually adding Bubble is scraped in oil stirring inflation, is carried out roughing, is collected graphite rougher concentration and mine tailing;The concentrate addition waterglass stirring of roughing acquisition, Add kerosene stirring, addition terpenic oil to stir and inflate and scrape bubble, carry out primary cleaning, collect selected concentrate;The essence of primary cleaning The stirring of ore deposit addition waterglass, the stirring of addition kerosene, addition terpenic oil are stirred and inflated and scrape bubble, and progress recleaning collects flotation Graphite concentrate;Above-mentioned flotation graphite concentrate adds NaOH solution to carry out batch mixing, is calcined, is washed to neutrality, with hydrochloric acid acidleach, washes, Dewatered drying, obtains graphite and fixes the high-carbon graphite product that carbon content reaches 98.74%;The purity of this method of purification does not reach More than 99.90%, and operating method is excessively complicated, cost is high.
Patent No. CN90109672.5, a kind of entitled method for purifying high-carbon graphite, during application (patent right) is artificial Xi'an optical precision optical machinery research institute of the academy of sciences of state, its technical scheme is:Using by hydrochloric acid, nitric acid (or sulfuric acid) and hydrofluoric acid group Into mixed acid agent, under normal temperature (0 DEG C -65 DEG C), the raw material of low-carbon grade 2-4 days in wet-treating, remove impurity, produce and carry Pure high-carbon graphite, the composition and its consumption of its mixed acid agent be according to the ore body composition of graphite raw material and the composition of ash content and its Content difference and prepare, based on every hectogram graphite raw material, the excursion of each composition usage amount of mixed acid agent is:Concentrated hydrochloric acid 15-60ml, concentrated nitric acid (or concentrated sulfuric acid) 0-30ml, hydrofluoric acid (40%) 15-60ml above-mentioned various sour agent allow to change in proportion Calculation uses diluted acid, can be separately added into, and can also be added with mixed acid, and water (or spent acid mother liquor) can then make as supplement Obtain solution and flood graphite raw material, somewhat excessive to be advisable, daily stirring is for several times.This operating method is excessively complicated, and cost is high, and the time It is long.
The content of the invention
There is provided that a kind of cost is low, steady quality it is an object of the invention to overcome above-mentioned weak point of the prior art Micro crystal graphite high-temperature fluorination method of purification.
The present invention is realized in the following way:
A kind of micro crystal graphite high-temperature fluorination method of purification, it is characterised in that:It is 1 to take weight ratio:0.7-1.48 fixed carbon For 99.9% natural micro crystal graphite and fluorization agent, deliver to and pyroreaction is carried out in serialization high temperature furnace, temperature is 2800-3000 DEG C, reaction time 10-60min obtains the natural micro crystal graphite that purity is more than 99.990%.
Preferably, the fluorization agent is one kind in poly- carbon tetrachloride, polytetrafluoroethylene (PTFE).
The beneficial effects of the present invention are:Using fluorization agent and serialization high temperature furnace, purification fixed carbon 99.9% graphite is extremely Fixed carbon 99.990-99.999% graphite;Fluorization agent causes the impurity in graphite to remove more completely;Serialization high temperature furnace was operated Journey can serialization, the error of reduction human factor.
Embodiment
The specific embodiment of the invention is now described in detail:
A kind of micro crystal graphite high-temperature fluorination method of purification, it is characterised in that:It is 1 to take weight ratio:0.75-1.45 fixed carbon For 99.9% natural micro crystal graphite and fluorization agent, deliver to and pyroreaction is carried out in serialization high temperature furnace, temperature is 2800-3000 DEG C, reaction time 10-60min obtains the natural micro crystal graphite that purity is more than 99.990%.
Fluorization agent of the present invention is one kind in poly- carbon tetrachloride, polytetrafluoroethylene (PTFE).
Embodiment 1
The natural micro crystal graphite 30kg that fixed carbon 99.9% is is taken, poly- carbon tetrachloride 22.5-43.5kg is added, delivered to continuous Change and pyroreaction is carried out in high temperature furnace, temperature is 2800-3000 DEG C, reaction time 30-60min, and being fixed carbon is 99.9992% high-purity natural micro crystal graphite.
Embodiment 2
It is natural micro crystal graphite 50kg to take fixed carbon 99.9%, adds polytetrafluoroethylene (PTFE) 37.5-72.5kg, delivers to serialization Pyroreaction is carried out in high temperature furnace, temperature is 2800-3000 DEG C, reaction time 30-60min, and it is 99.9992% to be fixed carbon High-purity natural micro crystal graphite.
Carbon content is fixed in the sample of two embodiments of the above, graphite products Quality Supervision and Inspection Center of warp let-off country Detection, specific testing result is as follows:
Therefore, by present invention fluorization agent and serialization high temperature furnace the purification graphite of fixed carbon 99.9% can be realized to admittedly Determine carbon 99.990-99.999% graphite.

Claims (2)

1. a kind of micro crystal graphite high-temperature fluorination method of purification, it is characterised in that:It is 1 to take weight ratio:0.7-1.48 fixed carbon is 99.9% natural micro crystal graphite and fluorization agent, delivers to and pyroreaction is carried out in serialization high temperature furnace, temperature is 2800-3000 DEG C, reaction time 10-60min obtains the natural micro crystal graphite that purity is more than 99.990%.
2. a kind of micro crystal graphite high-temperature fluorination method of purification according to claim 1, it is characterised in that:The fluorization agent is One kind in poly- carbon tetrachloride, polytetrafluoroethylene (PTFE).
CN201710293844.3A 2017-04-28 2017-04-28 A kind of micro crystal graphite high-temperature fluorination method of purification Pending CN106966388A (en)

Priority Applications (1)

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CN201710293844.3A CN106966388A (en) 2017-04-28 2017-04-28 A kind of micro crystal graphite high-temperature fluorination method of purification

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112028069A (en) * 2020-08-27 2020-12-04 中南钻石有限公司 Preparation and method for purifying waste graphite in industrial diamond production

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102602908A (en) * 2012-04-09 2012-07-25 上海尚饮思生化医药有限公司 Purification method of battery-grade graphite fluoride
CN104211048A (en) * 2013-06-05 2014-12-17 中国科学院上海有机化学研究所 Preparation method of fluorinated graphene

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102602908A (en) * 2012-04-09 2012-07-25 上海尚饮思生化医药有限公司 Purification method of battery-grade graphite fluoride
CN104211048A (en) * 2013-06-05 2014-12-17 中国科学院上海有机化学研究所 Preparation method of fluorinated graphene

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
付甲尧: ""通气石墨化机理的探讨"", 《碳素》 *
胡祥龙等: ""连续式高温反应石墨提纯装备与工艺"", 《新型炭材料》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112028069A (en) * 2020-08-27 2020-12-04 中南钻石有限公司 Preparation and method for purifying waste graphite in industrial diamond production
CN112028069B (en) * 2020-08-27 2021-12-10 中南钻石有限公司 Preparation and method for purifying waste graphite in industrial diamond production

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Application publication date: 20170721

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